液相色谱化学发光检测法的新进展

本文评述了近年来液相色谱化学发光检测法的新进展，内容涉及各类化学发光发反应，生物发光反应和电致化学发光反应同色谱体系的偶合方式，仪器设计，多种无机，有机，生物大分子和生物活性物质的分析方法及其在环境，生物医学科学和生命科学中的应用和发展方向。引用文献１６８篇。     

液相色谱-化学发光检测法的最新进展

评述了近年来液相色谱－化学发光检测法的最新进展,参考文献从１９９２年到１９９５年。内容涉及各类化学发光反应同液相色谱体系的耦合方式,仪器设计,多种无机、有机、生物大分子、生物活性物质及药物的分析方法及其在环境、生物医学科学和生命科学、临床化学及药物化学中的应用和发展方向。     

一种新的液相色谱检测器——抑制化学发光反应检测器

化学发光分析法以其仪器设备简单、操作方便、分析快速、灵敏度高、线性浓度范围宽等显著优点,引起人们极大的兴趣。然而,由于化学发光反应固有的选择性差的缺点,使得这种高灵敏检测方法在分析应用中受到很大限制。如何将高灵敏度的化学发光检测法与高选择性的物理或化学手段相结合,这     

化学发光消耗型锰传感器

化学和生物发光是由化学反应产生的一种光辐射,不需要任何光源。又由于它们具有高灵敏度、宽线性范围和相对比较便宜的仪器等优点,因而在化学和生物传感器领域引起了广泛的兴趣。已用于H_2O_2、乳酸和胆固醇等多种生物活性物质的测定,但未见有金属离子传感器的报道。本文发展了一种新型的全固态模式的消耗型锰离子化学发光传感器。该传感器将除待测物外的所有化学发光反应试剂全部固定在阴离子交换树脂Amberlyst A-27上,于化学发光反应之前,将一定量化学发光试剂从固定化试剂柱上洗脱,与样品中的锰离子产生化学发光。已成功地应用于水样中痕量锰离子的测定。每个固定化试剂柱可连续使用100次以上。 1 实验部分 1.1 仪器和试剂 化学发光传感器由流动系统和检测系统两部分组成。其中流动系统主要由蠕动泵、六通阀、固定化试剂柱和流通池组成。检测系统由光电信增管、负高压、放大器和记录仪组成(图1)。     

发光分析

本文是《分析试验室》定期评述中“发光分析”课题的第四篇评述文章，它评述在１９９５年１月～１９９６年１２月间我国发光分析的发展概况，内容包括：荧光，磷光，化学发光和生物发光分析等方面，引用文献３５４篇。     

流动注射化学发光法测定异烟肼

报道一种微量测定抗结核药物剧烟的新方法，方法是基于异烟肼对鲁米诺－锰（Ⅱ）－高碘酸钾化学发光反应的增敏作用，建立了微量异烟肼流的流动注射化学发光分析法。     

MnO2纳米溶胶-甲醛化学发光体系及其分析应用研究

Na2S2O3在中性水溶液中还原KMnO4可制备得到暗棕色的可溶性MnO2溶胶.所制备的MnO2溶胶透明、稳定,最大吸收波长位于357 nm处,平均粒径约40 nm.研究发现,所制备的MnO2纳米溶胶在酸性介质中与甲醛反应可产生弱的化学发光.考察了近30种药物分子在MnO2纳米溶胶-甲醛体系中的化学发光行为.结果表明,吩噻嗪类药物、氨基硫醇类药物等对该体系的化学发光信号具有显著的增强作用.据此,建立了利用这一化学发光体系测定五种吩噻嗪类药物和四种氨基硫醇类药物新的流动注射化学发光分析方法.所建立的方法被成功地用于片剂中奋乃静含量和猪饲料中盐酸氯丙嗪含量的测定.通过对化学发光光谱、荧光光谱、紫外可见吸收光谱等实验的研究,提出了可能的化学发光反应机理.所有反应的化学发光光谱的最大发射波长均位于630～640 nm间,与分析物的种类无关.当向反应体系中加入单线态氧清除剂叠氮化钠和三亚乙基二胺时,反应的化学发光强度被不同程度的抑制,这表明单线态氧可能是该化学发光反应的发光体.     

苯二酚异构体的高效液相色谱化学发光检测法研究

高效液相色谱作为一种有效的分离手段已被用于酚类化合物的分析 ,紫外检测法 [1～ 3] 、电化学检测法[3,4 ] 等已用于苯二酚异构体的测定 ,但苯二酚异构体的化学发光检测法尚未见文献报道 .前文 [5] 结果表明 ,苯二酚异构体等对鲁米诺诱导的化学发光具有很强的抑制作用 .基于此 ,本文将高效液相色谱与化学发光技术联用 ,首次建立了苯二酚异构体的高效液相色谱化学发光检测法 .该法灵敏度高 ,选择性好 ,为酚类物质的测定提供了一条新的途径 .1　实验部分1 .1　仪器与试剂　 FIA- 2 4 0 0型流动注射分析仪 (中国科学院信通科学仪器公司 ) ;G…     

化学发光分析法应用进展

对近年来化学发光分析法的研究应用最新进展作了评述，包括化学发光试剂的类型，化学发光在无机、有机及药物分析中的应用，全文引用文献105篇。     

鲁米诺的合成与振荡化学发光

鲁米诺的合成与化学发光是一个极具展示度的基础化学实验。近年来，国内部分高校陆续开设了这一实验，引起不错的反响。为进一步丰富和提升该实验的科学理论内涵，我们进行了如下改进：1)在合成部分引入机械搅拌、硫粉还原和微波合成，实现安全、快速、高效制备高纯度鲁米诺的目的；2)在单次化学发光的基础上，特别引入宛如星辰闪烁般的振荡化学发光反应(鲁米诺/H2O2/SCN-/Cu2+/OH-振荡体系)，该反应涉及非平衡态热力学和非线性化学等重要概念与基础理论知识，激发学生的求知欲；3)设计并搭建了可与荧光光谱仪配套使用的简易微型磁力搅拌加热装置，实现了对振荡化学发光的光强和振荡周期等数据的实时定量监测，使学生可以自行设计对比实验，探究影响振荡反应过程的因素，并总结振荡反应规律。该实验涵盖了多学科的重要知识点，兼具科学性与趣味性，对培养学生的探索精神和创新意识具有重要意义。     

Comparison of traditional cloud-point extraction and on-line flow-injection cloud-point extraction with a chemiluminescence method using benzo[a]pyrene as a marker

In this work, using benzo(a)pyrene (BaP) as marker, the analytical merits of on-line flow-injection cloud-point extraction (FI CPE), including preconcentration factor, extraction efficiency, sample throughput, and analysis time were evaluated by use of peroxyoxalate chemiluminescence (CL) detection. Moreover, by detailed discussion of several preconcentration conditions for traditional and on-line FI CPE the advantages of on-line FI CPE became conspicuously apparent. When coupled with separation techniques such as high-performance liquid chromatography (HPLC) or capillary electrophoresis (CE), on-line FI CPE–CL has much potential for analysis of low concentrations of polycyclic aromatic hydrocarbons (PAH) in environmental samples.     

Chemiluminescence flow sensor for folic acid with immobilized reagents.

A novel chemiluminescence (CL) sensor for folic acid combined flow-injection (FI) technology was presented in this paper. The analytical reagents involved in the CL reaction, including luminol and hexacyanoferrate(III), were both immobilized on an anion-exchange column in FI system. The CL signal produced by the reaction between luminol and hexacyanoferrate(III), which were eluted from the column through sodium phosphate injection, was decreased in the presence of folic acid. The CL emission was correlated with the folic acid concentration in the range from 0.01 to 15 microg ml(-1), and the detection limit was 3.5 ng ml(-1) folic acid (3sigma). At a flow rate of 2.0 ml min(-1), including sampling and washing, could be performed in 2 min with a relative standard deviation of < 2.5%. The flow sensor could be reused more than 300 times and has been applied to the analysis of folic acid in pharmaceutical preparations. and the recovery was from 97.4% to 100.4%.     

Determination of Picogram Amounts of Dihydroxybenzenes in Water Samples with Luminol–lysozyme Chemiluminescence System

An ultrasensitive method for the determination of dihydroxybenzens by flow injection (FI) chemiluminescence (CL) analysis was proposed for the first time. It was found that the CL intensity of luminol–lysozyme system could be significantly inhibited by dihydroxybenzens. The CL intensity decrements were linear with the logarithm of dihydroxybenzens concentrations over the ranges of 1.0 ～ 700 pg mL^‐1 for hydroquinone (HQ), 5.0 ～ 700 pg mL^‐1 for catechol (CT) and 10 ～ 7000 pg mL^‐1 for resorcinol (RS), with the corresponding limits of detection of 0.7, 3.0 and 7.0 pg mL^‐1, respectively. The proposed method was successfully applied to the determination of CT in tap water, rain water, river water and HQ in waste photographic developer samples, with recoveries from 93.5 to 105.8% and relative standard deviations (RSDs) less than 4.0% (n = 5). The possible interaction mechanism of lysozyme with dihydroxybenzens was discussed, and CT to lysozyme's binding constant and the thermodynamic parameters were given by the homemade FI–CL model. The results shown that the binding of dihydroxybenzens to lysozyme was spontaneous with the hydrophobic force.     

Chemiluminescent Determination of Inorganic Phosphate

Flow injection (FI) chemiluminescence (CL) analysis has received much attention in various fields for its high sensitivity, rapidity, simplicity and feasibility. Recently, interest has also focused on the use of FI in site monitoring of environmental materials in surface and sea water, such as phosphate. Most of the commonly used methods for the determination of inorganic phosphate by FI are based on spectrophotometric measurement of the phosphomlybate or phosphomolybdovanadate complex^[1], or fluorescence quenching methods using metals, such as aluminium-morin (Al-morin) system^[2]. A new CL determination of inorganic phosphate by FI system is described (Fig 1).     

Capillary electrophoresis system with flow injection sample introduction and chemiluminescence detection on a chip platform

A capillary electrophoresis (CE) system with chemiluminescence (CL) detection was combined with flow injection (FI) sample introduction on a chip platform. A falling-drop interface was applied to perform FI split-flow sample introduction while achieving electrical isolation from the CE high voltage. A tubular reservoir at the capillary outlet served as both the CL reaction and detection cell for the luminol-peroxide-metallic ion chemiluminescent reaction, with the luminol included in the separation buffer and CL reagent H2O2 continuously introduced into the outlet reservoir. An optical fiber was positioned within the outlet reservoir directly opposite, and 300 microns away from, the capillary outlet for collecting and transferring the generated CL to the PMT. The peak height signals and the separation efficiency were almost independent of the reagent flow-rate, making the system a robust one. The performance of the system was illustrated by the separation of Co(II) and Cu(II), achieving baseline separation in 60 s. Detection limits (3 sigma) were 1.25 x 10(-8) and 2.3 x 10(-6) mol dm-3 for Co(II) and Cu(II), respectively. Peak height precision was 1.9% RSD (n = 9) at the 10(-7) mol dm-3 Co level.     

Solid Phase Extraction Chemiluminescence Determination of Methamidaphos on Vegetables

IntroductionDuring recent years,organophosphorus pesticides(OPPs)have been widely used in agriculture becauseof their low environmental persistence and high effec-tiveness.However,they have a high acute toxicity.Trace amounts of OPPs may remain in foodstu…     

Characterization of a micro spiral flow cell for chemiluminescence detection

A 5.5 μl spiral micro-flow cell, mounted in front of a photomultiplier, is made from Teflon capillary (75 cm×100 μm ID) with two inlets for the CL reagent and carrier buffer and a waste outlet. It allows the rapid mixing of CL reagent and analyte and simultaneous detection of the emitted light. Using a flow rate of 25 μl/min for a 0.4 mM luminol-8 μM hemin solution (pH 11.6) and 50 μl/min of carrier buffer (pH 11.6), the slight exponential calibration curve for the flow injection–chemiluminescence (FI–CL) determination of H₂O₂ is 2.5–10 μM and the detection limit is 1.5 μM. The detection limit achieved by using a spiral flow cell is 24 times lower than that obtained from a conventional FI system with a low dead volume tee mixer and a 12 μl flow cell in a HPLC fluorometer with the source lamp off. This luminol CL detection method is successfully applied to the enzymatic determination of -lactate by FI. The lactate sample is mixed with polyethylene glycol (PEG)-stabilized lactate oxidase (LO) enzyme and then injected into the buffered (pH 7.5) carrier stream for CL detection of the H₂O₂ product. Using the optimal conditions of reaction temperature set to 37.5 °C and flow rates of 45 μl/min for the CL reagent and 60 μl/min for the carrier buffer, the calibration range for lactate is 5–50 μM and the detection limit is 2.9 μM. This method is applied to the determination of -lactate in beer.     

Determination of Total Chromium in Biological Samples by Automated Reagent Injection Chemiluminescence Analysis

A sensitive method for the determination of total chromium in real samples by flow injection–chemiluminescence (FI–CL) analysis was proposed. It was found that the CL intensity from luminol–lysozyme reaction could be markedly quenched, and the decrease of CL intensity was linear with the logarithm of Cr(III) concentrations over the range of 5.0 to 4000 pg mL^?1 with a detection limit of 2.0 pg mL^?1 (3σ) and relative standard deviations (RSDs) of 3.0, 2.6, and 2.0% for 10, 100, and 1000 pg mL^?1 Cr(III) (n = 7), respectively. At a flow rate of 2.0 mL min^?1, the whole process including sampling and washing could be accomplished within 36 s. The proposed CL method was successfully applied to the determination of total chromium in pharmaceutical capsules, a dietary supplement, and spiked human serum samples, with recoveries from 92.2 to 108.4% and RSDs of less than 4.0%. Using the homemade FI–CL model, the binding constant (K = 4.38 × 10⁶ L mol^?1) and the binding sites (n ≈ 1) of Cr(III) to lysozyme were given.     

Sensitive Determination of Nanogram Levels of Diacerein in a Pharmaceutical Formulation by Flow Injection Chemiluminescence Analysis

A simple, sensitive and inexpensive flow injection chemiluminescence (FI‐CL) method for the determination of diacerein was proposed. It was based on the greatly enhancive effect of diacerein on the CL reaction between luminol and hydrogen peroxide in alkaline medium. The enhanced CL intensity was linear with the concentration of diacerein over the range 1.0–500 ng/mL with a detection limit (3σ) of 0.2 ng/mL. The relative standard deviation was 1.1% (n = 8, 20 ng/mL diacerein) and the sample throughput was about 120 samples h^?1. This simple method has been successfully applied for the determination of diacerein in a pharmaceutical formulation without interference from its potential impurities. The degradation of diacerein was also investigated briefly.     

Electrogeneration of ferrate (VI) in low concentration NaOH solution for flow injection–chemiluminescence detection

The possibility of direct analytical applications of ferrate(VI) solution, which was freshly electrogenerated in low-concentration NaOH electrolyte, was studied by a flow-injection chemiluminescence (FI–CL) system. It was found that some inorganic ions, organic molecule and biomolecule could enhance the chemiluminescence emission caused by ferrate(VI)–luminol reaction. V(V), Ca(II), Mg(II), phloroglucinol, and bovine hemoglobin (Hb) chosen as samples were successfully detected by this developed method. The analytical characteristics of the system for the analytes determination including linear ranges, correlation coefficients, limits of detection combined with FI analysis were studied.